CN102241706B - D-ribose purification and separation method - Google Patents
D-ribose purification and separation method Download PDFInfo
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Abstract
The invention relates to a D-ribose purification and separation method, comprising the following steps of: 1) filtering a D-ribose broth with a flat membrane with a molecular weight cut-off of 10,000-15,000, and sending the flat membrane filtrate into an anticlockwise rotated ion exchange resin column continuously moving bed; 2) sending a lower column liquid from the ion exchange resin column continuously moving bed to an anticlockwise rotated anion exchange resin column continuously moving bed; 3) concentrating a lower column liquid from the anion exchange resin column continuously moving bed to a concentration of 18-25%, and then sending a concentrate to an anticlockwise rotated gel chromatogram separation continuously moving bed; 4) collecting a lower column liquid from a D-ribose washing zone of the gel chromatographic separation continuously moving bed to obtain a purified D-ribose product. The method combines a membrane filtration technology, a continuous ion exchange technology and a continuous chromatogram technology to obtain a D-ribose with a purity and yield higher than those of a D-ribose from a prior purification and separation method.
Description
Technical field
The present invention relates to a kind of method for purifying and separating, relate to particularly a kind of method for purifying and separating of D-ribose.
Background technology
D-ribose is natural aldopentose, be present in all viable cell, be the important component part of vector rna, DNA and the Nucleotide of genetic information in life cells, significant to vital movement, and all have a wide range of applications at industrial sectors such as medicine, food, feeds.The production method of D-ribose has three kinds: a kind of is separation and Extraction from yeast nucleic acid; The 2nd, take glucose, pectinose to obtain as the method for raw material by chemosynthesis; The 3rd, use glucose is raw material, and with obtaining after the fermentation of transketolase deficient strain, and the most common with the third.But, owing to containing the macromole impurity such as different kinds of ions, pigment and five-carbon sugar, hexose and its phosphoric acid ester and albumen in fermented liquid, cause D-ribose separation, purify extremely difficult.The following step of the general employing of existing purifying technique: the centrifugal thalline of removing of fermented liquid, with activated carbon decolorizing, then remove the zwitterion in fermented liquid by ion-exchange, through concentrating under reduced pressure, with the ethanol precipitated crystal of 4 times of volumes, obtain product.But, in above-mentioned technique, owing to failing to remove the small-molecule substances such as five-carbon sugar in fermented liquid, hexose, cause the purity of D-ribose crystallization lower.In addition, a kind of method of utilizing membrane separation technique separation and Extraction D-ribose from fermented liquid is disclosed in CN1266158C, in the method, the nanofiltration membrane that D-ribose fermented liquid is 300～800 by aperture is the filter membrane of 3～10 μ m, microfiltration membrane that aperture is 02～0.5 μ m, molecular weight cut-off is 3000～10000 ultrafiltration membrance filter and molecular weight cut-off is successively filtered, then again nanofiltration membrane filtered liquid is carried out to ion-exchange, concentrated, crystallization, make purity and reach 99% D-ribose.But above-mentioned mode not only operation steps is extremely complicated, length consuming time, and D-ribose yield is low.
Summary of the invention
The method for purifying and separating that the object of this invention is to provide a kind of D-ribose, to solve the above-mentioned problems in the prior art.The method comprehensive membrane filters, continuously from handing over and continuous chromatography technology, make separated after the purity of D-ribose and yield far away higher than existing method for purifying and separating.
Technical scheme provided by the invention is as follows:
A method for purifying and separating for D-ribose, is characterized in that, comprises following step:
1) by D-ribose fermented liquid molecular weight cut-off, be that 10,000～15,000 flat sheet membrane is filtered, the filtered liquid of flat sheet membrane sent into the cation exchange resin column Continuous Moving Bed rotating counterclockwise;
2) several cation exchange resin columns of Continuous Moving Bed are divided in the direction of the clock successively to mixed solution intake zone, Xi Suan district and five, the acid regeneration district subregion of water liftout district, flat sheet membrane filtered liquid intake zone, Gai Shui liftout district liftout water and this intake zone lower column liquid, collect the outlet of parallel feeding district and remove cationic lower column liquid, lower column liquid is sent into the anion-exchange resin column Continuous Moving Bed rotating counterclockwise;
3) several anion-exchange resin columns of Continuous Moving Bed are divided into water liftout district, the mixed solution intake zone that removes cationic lower column liquid intake zone, Gai Shui liftout district liftout water and this intake zone lower column liquid, five of He Jian breeding blankets, soda district subregion in the direction of the clock successively, collect the lower column liquid that the outlet of parallel feeding district removes negatively charged ion;
4) lower column liquid in step 3 is concentrated into 18～25% concentration, then concentrated solution is sent into the gel-type chromatographic separation resin column Continuous Moving Bed rotating counterclockwise;
5) several gel-type chromatographic separation resin columns of Continuous Moving Bed are divided into D-ribose elution zone, prolongation disengaging zone and three of the impurity disengaging zone subregion with salt-free water elution in the direction of the clock successively, the lower column liquid of D-ribose elution zone enters one first batch can, feed liquid in the first batch can enters prolongation disengaging zone from extending the ingress of disengaging zone, then from extending the exit of disengaging zone, flows into one second batch can again; In the second batch can, supplement pending fresh concentrated solution, mixing solutions in the second batch can enters impurity disengaging zone from the ingress of impurity disengaging zone, then from the exit of impurity disengaging zone, flow into one the 3rd batch can again, the feed liquid in the 3rd batch can is discharged as waste water; The feed liquid of collecting in the first batch can is D-ribose product.
In the embodiment recommending, the working pressure of flat sheet membrane is controlled at 1～6bar, and temperature is controlled at 20～80 ℃.
In the embodiment recommending, in step 2, water liftout district comprises 2～3 resin columns that are connected in series, flow rate of liquid is 25～35mL/min, intake zone comprises 2～3 resin columns that are connected in series, flow rate of liquid is 90～100mL/min, mixed solution intake zone comprises whole series connection, 4～5 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 110～140mL/min, Xi Suan district comprises whole series connection, 5～7 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 45～55mL/min, acid regeneration district comprises 4～6 resin columns that are connected in series, flow rate of liquid is 35～45mL/min, cation exchange resin column Continuous Moving Bed system amount of resin is 5～12L, the rotating disk cycle is 500～650min.
In the embodiment recommending, in step 3, water liftout district comprises 2～3 resin columns that are connected in series, flow rate of liquid is 25～35mL/min, intake zone comprises 2～3 resin columns that are connected in series, flow rate of liquid is 60～80mL/min, mixed solution intake zone comprises whole series connection, 4～5 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 90～110mL/min, soda district comprises whole series connection, 5～7 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 50～70mL/min, alkali breeding blanket comprises 4～6 resin columns that are connected in series, flow rate of liquid is 35～45mL/min, anion-exchange resin column Continuous Moving Bed system amount of resin is 5～12L, the rotating disk cycle is 500～650min.
In the embodiment recommending, in step 4, use reverse osmosis membrane concentrated the parallel feeding district lower column liquid obtaining in step 3, it is that the nanofiltration membrane of 1～5nm is concentrated that the concentrated solution of reverse osmosis membrane re-uses aperture, obtain the lower column liquid of 18～25% concentration, it is again concentrated that the dialyzate of nanofiltration membrane is sent reverse osmosis membrane again back to.
In the embodiment recommending, several gel-type chromatographic separation resin columns of Continuous Moving Bed are divided into D-ribose elution zone, prolongation disengaging zone, impurity disengaging zone and assorted four subregions of sugared enrichment region in the direction of the clock successively, and the feed liquid in the 3rd batch can is entered to assorted sugared enrichment region from the ingress of assorted sugared enrichment region, then from the outlet of assorted sugared enrichment region, flow out, the feed liquid of outflow is discharged as waste water again.
In the embodiment recommending, in step 5, the feed liquid take-off rate of the second batch can is identical with the feed liquid of the second batch can inflow flow velocity.
In the embodiment recommending, in step 5, D-ribose elution zone comprises 5～6 resin columns that are connected in series, flow rate of liquid is 59～62mL/min, extend disengaging zone and comprise 5～6 resin columns that are connected in series, flow rate of liquid is 44～45mL/min, impurity disengaging zone comprises 5～6 resin columns that are connected in series, flow rate of liquid is 51～53mL/min, assorted sugared enrichment region comprises 5～6 resin columns that are connected in series, flow rate of liquid is 23～26mL/min, gel-type chromatographic separation resin column Continuous Moving Bed system amount of resin is 8～16L, the rotating disk cycle is 200～300min.
Compared with prior art, method for purifying and separating provided by the invention has following feature:
1, the method comprehensive membrane filter, continuously from handing over and continuous chromatography technology, make separated after the purity of D-ribose and yield far away higher than existing method for purifying and separating;
2, the D-ribose extraction system in the method operates steadily, and operating parameters is stable;
3, flat sheet membrane can reach the effect of removal of impurities preferably, its film core operating flux is stable, cycles of concentration can reach more than 40 times, and film core cleans easily, adopt clean-out system to clean and can recover the initial flux of film core, for effective constituent is taken out of as far as possible, reduce product loss, in filtration procedure, can add a small amount of water (be generally charging 5%～30%);
4, compare with resin fixed bed, the resin Continuous Moving Bed that the present invention uses can be saved resin over half, reduces organic solvent usage quantity, and the concentration of product can be improved, and saves the evaporation concentration cost of subsequent technique;
5, present method adopts the concentrated D-ribose of membrane technique from handing over lower column liquid, the more existing more environmental protection of mode that utilizes evaporation concentration, energy-conservation, efficient.
Accompanying drawing explanation
Fig. 1 is the use state graph of the Zeo-karb Continuous Moving Bed of the embodiment of the present invention;
Fig. 2 is the use state graph of the anionite-exchange resin Continuous Moving Bed of the embodiment of the present invention;
Fig. 3 is the use state graph of the gel-type chromatographic separation resin column Continuous Moving Bed of the embodiment of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but do not form any limitation of the invention.
Embodiment 1
One, flat sheet membrane is filtered
The D-ribose fermented liquid molecular weight cut-off that is 6% by D-ribose content is that 10,000～15,000 flat sheet membrane is filtered, and import operation pressure-controlling is at 2～3bar, top hole pressure 1～1.5bar, and 30～45 ℃ of temperature, average flux is 133～138LMH.In process of the test, to the sampling of film dialyzate, detect total nitrogen index, result demonstration, the total nitrogen index in dialyzate is 0.
Detect charging D-ribose total amount and discharging D-ribose total amount, result demonstration, D-ribose yield is 98.0%.
The filtered liquid of flat sheet membrane is sent into the cation exchange resin column Continuous Moving Bed rotating counterclockwise.
Two, cation exchange resin column Continuous Moving Bed Liquidity limit
As shown in fig. 1, cation exchange resin column Continuous Moving Bed is provided with 20 resin columns, the water liftout district 101 that is divided into successively in the direction of the clock salt-free water elution, flat sheet membrane filtered liquid intake zone 102, mixed solution intake zone 103, 105 5, Xi Suan district 104He acid regeneration district subregion, this wherein, 1st～No. 3 Zhu Weishui liftout districts 101 that are connected in series, 4th～No. 5 posts that are connected in series are filtered liquid intake zone 102, after the liftout water in Gai Shui liftout district 101 and the lower column liquid of filtered liquid intake zone 102 mix in a batch can, send into the mixed solution intake zone 103 being formed by 6th～No. 9 posts, it adopts following mode of connection (6, 7)-(8, 9), 10th～No. 15 Zhu Weixisuan districts 104 (use without salt solution and clean), and adopt following mode of connection 10-11-(12, 13)-(14, 15), 16th～No. 20 Zhu Wei acid regeneration districts 105 that are connected in series.
The flow rate of liquid in water liftout district 101 is 25mL/min, and its import is arranged on the upper end opening for feed of No. 1 post, and its outlet is arranged on the lower end discharge port of No. 3 resin column; The flow rate of liquid of filtered liquid intake zone 102 is 90mL/min, and its import is arranged on the upper end opening for feed of No. 4 post, and its outlet is arranged on the lower end discharge port of No. 5 resin column; The flow rate of liquid of mixed solution intake zone 103 is 110mL/min, and its import is arranged on the upper end opening for feed of the 6th, No. 7 posts, and its outlet is arranged on the lower end discharge port of the 8th, No. 9 resin columns, collects its lower column liquid; The flow rate of liquid in Xi Suan district 104 is 45mL/min, and its import is arranged on the upper end opening for feed of No. 10 post, and its outlet is arranged on the lower end discharge port of the 14th, No. 15 resin columns; The flow rate of liquid in acid regeneration district 105 is 35mL/min, and its import is arranged on the upper end opening for feed of No. 16 post, and its outlet is arranged on the lower end discharge port of the 19th, No. 20 resin columns.
The turntable rotation cycle of controlling cation exchange resin column Continuous Moving Bed is 500min.
After turntable rotation two weeks, continuous moving bed system is balanced, detect the lower column liquid of No. 1 post in water liftout district 101, the D-ribose concentration of No. 1 post lower column liquid is 0.03%, the loss of D-ribose is minimum, by calculating D-ribose total amount in charging D-ribose total amount, discharging D-ribose total amount and transfer charging basket, investigates material balance situation, result demonstration, D-ribose yield is 98.5%.
The lower column liquid of mixed solution intake zone 103 is sent into anion-exchange resin column Continuous Moving Bed.
Three, anion-exchange resin column Continuous Moving Bed adsorpting anion
As shown in Figure 2, anion-exchange resin column Continuous Moving Bed is provided with 20 resin columns, the water liftout district 201 that is divided into successively in the direction of the clock salt-free water elution, the intake zone 202 of parallel feeding district 103 lower column liquids, the mixed solution intake zone 203 of liftout water and intake zone 202 lower column liquids, 205 5 of 204He Jian breeding blankets, soda district subregion, this wherein, 1st～No. 3 Zhu Weishui liftout districts 201 that are connected in series, 4th～No. 5 posts that are connected in series are filtered liquid intake zone 202, after the lower column liquid of Gai Shui liftout district 201 and dull and stereotyped membrane filtration liquid intake zone 202 mixes in a batch can, send into the mixed solution intake zone 203 being formed by 6th～No. 9 posts, it adopts following mode of connection (6, 7)-(8, 9), 10th～No. 15 Zhu Wei soda districts 204 (use without salt solution and clean), and adopt following mode of connection 10-11-(12, 13)-(14, 15), 16th～No. 20 Zhu Weijian breeding blankets 205 that are connected in series.
The flow rate of liquid in water liftout district 201 is 25mL/min, and its import is arranged on the upper end opening for feed of No. 1 post, and its outlet is arranged on the lower end discharge port of No. 3 resin column; The flow rate of liquid of filtered liquid intake zone 202 is 60mL/min, and its import is arranged on the upper end opening for feed of No. 4 post, and its outlet is arranged on the lower end discharge port of No. 5 resin column; The flow rate of liquid of mixed solution intake zone 203 is 90mL/min, and its import is arranged on the upper end opening for feed of the 6th, No. 7 posts, and its outlet is arranged on the lower end discharge port of the 8th, No. 9 resin columns, collects its lower column liquid; The flow rate of liquid in soda district 204 is 50mL/min, and its import is arranged on the upper end opening for feed of No. 10 post, and its outlet is arranged on the lower end discharge port of the 14th, No. 15 resin columns; The flow rate of liquid of alkali breeding blanket 105 is 35mL/min, and its import is arranged on the upper end opening for feed of No. 16 post, and its outlet is arranged on the lower end discharge port of the 19th, No. 20 resin columns.
The turntable rotation cycle of controlling anion-exchange resin column Continuous Moving Bed is 600min.
After turntable rotation two weeks, continuous moving bed system is balanced, detect the lower column liquid of No. 1 post in water liftout district 201, the D-ribose concentration of No. 1 post lower column liquid is 0.03%, the loss of D-ribose is minimum, by calculating D-ribose total amount in charging D-ribose total amount, discharging D-ribose total amount and transfer charging basket, investigates material balance situation, result demonstration, D-ribose yield is 98.2%.
The lower column liquid of mixed solution intake zone 203 is sent into concentration systems.
Four, reverse osmosis membrane and nanofiltration membrane are concentrated
Use reverse osmosis membrane concentrated parallel feeding district lower column liquid in anion-exchange resin column Continuous Moving Bed, it is that the nanofiltration membrane of 1～5nm is concentrated that the concentrated solution of reverse osmosis membrane re-uses aperture, obtain the lower column liquid of 18% concentration, it is again concentrated that the dialyzate of nanofiltration membrane is sent reverse osmosis membrane again back to.Concentrated solution is sent into the gel-type chromatographic separation resin column Continuous Moving Bed rotating counterclockwise.
Five, gel-type chromatographic separation resin column Continuous Moving Bed is separated
As shown in Figure 3, gel-type chromatographic separation resin column Continuous Moving Bed is provided with 20 resin columns, and is divided into successively in the direction of the clock D-ribose elution zone 301, prolongation disengaging zone 302, impurity disengaging zone 303 and assorted 304 4 subregions of sugared enrichment region with salt-free water elution.This wherein, 1st～No. 5 posts that are connected in series are D-ribose elution zone 301, enter feed liquid in one first batch can 1, the first batch can 1 enter and extend disengaging zone 302 from extending the ingress of disengaging zone 302 from the lower column liquid of D-ribose elution zone 301; 6th～No. 10 posts that are connected in series are for extending disengaging zone 302, the lower column liquid that extends disengaging zone 302 enters one second batch can 2, to the interior supplementary pending fresh concentrated solution of the second batch can 2, the mixing solutions in the second batch can 2 enters impurity disengaging zone 303 from the ingress of impurity disengaging zone 303; 11st～No. 15 posts that are connected in series are impurity disengaging zone 303, and the feed liquid that the lower column liquid of impurity disengaging zone 303 enters in one the 3rd batch can 3, the three batch cans 3 enters assorted sugared enrichment region 304 from the ingress of assorted sugared enrichment region 304; 16th～No. 20 posts that are connected in series are assorted sugared enrichment region 304, and the lower column liquid of assorted sugared enrichment region 304 is discharged as waste water.
The flow rate of liquid of D-ribose elution zone 301 is 59mL/min, and its import is arranged on the upper end opening for feed of No. 1 post, and its outlet is arranged on the lower end discharge port of No. 5 resin column; The flow rate of liquid that extends disengaging zone 302 is 44mL/min, and its import is arranged on the upper end opening for feed of No. 6 post, and its outlet is arranged on the lower end discharge port of No. 10 resin column; The flow rate of liquid of impurity disengaging zone 303 is 51mL/min, and its import is arranged on the upper end opening for feed of o.11 post, and its outlet is arranged on the lower end discharge port of No. 15 resin column; The flow rate of liquid of assorted sugared enrichment region 304 is 23mL/min, and its import is arranged on the upper end opening for feed of No. 16 post, and its outlet is arranged on the lower end discharge port of No. 20 resin column.
The feed liquid of collecting in the first batch can 1 is D-ribose product.
The turntable rotation cycle of controlling gel-type chromatographic separation resin column Continuous Moving Bed is 200min.
After turntable rotation two weeks, continuous moving bed system is balanced, detect the liquid material of the first batch can 1, the purity of D-ribose is 98%, the loss of D-ribose is minimum, by calculating charging D-ribose total amount and discharging D-ribose total amount, investigates material balance situation, result demonstration, D-ribose yield is 95.1%.
One, flat sheet membrane is filtered
The D-ribose fermented liquid molecular weight cut-off that is 6% by D-ribose content is that 10,000～15,000 flat sheet membrane is filtered, and import operation pressure-controlling is at 2～3bar, top hole pressure 1～1.5bar, and 40～50 ℃ of temperature, average flux is 135～138LMH.In process of the test, to the sampling of film dialyzate, detect total nitrogen index, result demonstration, the total nitrogen index in dialyzate is 0.
Detect charging D-ribose total amount and discharging D-ribose total amount, result demonstration, D-ribose yield is 98.5%.
The filtered liquid of flat sheet membrane is sent into the cation exchange resin column Continuous Moving Bed rotating counterclockwise.
Two, cation exchange resin column Continuous Moving Bed Liquidity limit
As shown in fig. 1, cation exchange resin column Continuous Moving Bed is provided with 20 resin columns, the water liftout district 101 that is divided into successively in the direction of the clock salt-free water elution, flat sheet membrane filtered liquid intake zone 102, mixed solution intake zone 103, 105 5, Xi Suan district 104He acid regeneration district subregion, this wherein, 1st～No. 3 Zhu Weishui liftout districts 101 that are connected in series, 4th～No. 5 posts that are connected in series are filtered liquid intake zone 102, after the liftout water in water liftout district 101 and the lower column liquid of filtered liquid intake zone 102 mix in a batch can, send into the mixed solution intake zone 103 being formed by 6th～No. 9 posts, it adopts following mode of connection (6, 7)-(8, 9), 10th～No. 15 Zhu Weixisuan districts 104 (use without salt solution and clean), and adopt following mode of connection 10-11-(12, 13)-(14, 15), 16th～No. 20 Zhu Wei acid regeneration districts 105 that are connected in series.
The flow rate of liquid in water liftout district 101 is 35mL/min, and its import is arranged on the upper end opening for feed of No. 1 post, and its outlet is arranged on the lower end discharge port of No. 3 resin column; The flow rate of liquid of filtered liquid intake zone 102 is 100mL/min, and its import is arranged on the upper end opening for feed of No. 4 post, and its outlet is arranged on the lower end discharge port of No. 5 resin column; The flow rate of liquid of mixed solution intake zone 103 is 140mL/min, and its import is arranged on the upper end opening for feed of the 6th, No. 7 posts, and its outlet is arranged on the lower end discharge port of the 8th, No. 9 resin columns, collects its lower column liquid; The flow rate of liquid in Xi Suan district 104 is 55mL/min, and its import is arranged on the upper end opening for feed of No. 10 post, and its outlet is arranged on the lower end discharge port of the 14th, No. 15 resin columns; The flow rate of liquid in acid regeneration district 105 is 45mL/min, and its import is arranged on the upper end opening for feed of No. 16 post, and its outlet is arranged on the lower end discharge port of the 19th, No. 20 resin columns.
The turntable rotation cycle of controlling cation exchange resin column Continuous Moving Bed is 600min.
After turntable rotation two weeks, continuous moving bed system is balanced, detect the lower column liquid of No. 1 post in water liftout district 101, the D-ribose concentration of No. 1 post lower column liquid is 0.02%, the loss of D-ribose is minimum, by calculating D-ribose total amount in charging D-ribose total amount, discharging D-ribose total amount and transfer charging basket, investigates material balance situation, result demonstration, D-ribose yield is 98.4%.
The lower column liquid of mixed solution intake zone 103 is sent into anion-exchange resin column Continuous Moving Bed.
Three, anion-exchange resin column Continuous Moving Bed adsorpting anion
As shown in Figure 2, anion-exchange resin column Continuous Moving Bed is provided with 20 resin columns, the water liftout district 201 that is divided into successively in the direction of the clock salt-free water elution, the intake zone 202 of parallel feeding district 103 lower column liquids, the mixed solution intake zone 203 of liftout water and intake zone 202 lower column liquids, 205 5 of 204He Jian breeding blankets, soda district subregion, this wherein, 1st～No. 3 Zhu Weishui liftout districts 201 that are connected in series, 4th～No. 5 posts that are connected in series are filtered liquid intake zone 202, after the lower column liquid of Gai Shui liftout district 201 and dull and stereotyped membrane filtration liquid intake zone 202 mixes in a batch can, send into the mixed solution intake zone 203 being formed by 6th～No. 9 posts, it adopts following mode of connection (6, 7)-(8, 9), 10th～No. 15 Zhu Wei soda districts 204 (use without salt solution and clean), and adopt following mode of connection 10-11-(12, 13)-(14, 15), 16th～No. 20 Zhu Weijian breeding blankets 205 that are connected in series.
The flow rate of liquid in water liftout district 201 is 35mL/min, and its import is arranged on the upper end opening for feed of No. 1 post, and its outlet is arranged on the lower end discharge port of No. 3 resin column; The flow rate of liquid of filtered liquid intake zone 202 is 80mL/min, and its import is arranged on the upper end opening for feed of No. 4 post, and its outlet is arranged on the lower end discharge port of No. 5 resin column; The flow rate of liquid of mixed solution intake zone 203 is 110mL/min, and its import is arranged on the upper end opening for feed of the 6th, No. 7 posts, and its outlet is arranged on the lower end discharge port of the 8th, No. 9 resin columns, collects its lower column liquid; The flow rate of liquid in soda district 204 is 70mL/min, and its import is arranged on the upper end opening for feed of No. 10 post, and its outlet is arranged on the lower end discharge port of the 14th, No. 15 resin columns; The flow rate of liquid of alkali breeding blanket 105 is 45mL/min, and its import is arranged on the upper end opening for feed of No. 16 post, and its outlet is arranged on the lower end discharge port of the 19th, No. 20 resin columns.
The turntable rotation cycle of controlling anion-exchange resin column Continuous Moving Bed is 500min.
After turntable rotation two weeks, continuous moving bed system is balanced, detect the lower column liquid of No. 1 post in water liftout district 201, the D-ribose concentration of No. 1 post lower column liquid is 0.03%, the loss of D-ribose is minimum, by calculating D-ribose total amount in charging D-ribose total amount, discharging D-ribose total amount and transfer charging basket, investigates material balance situation, result demonstration, D-ribose yield is 98.1%.
The lower column liquid of mixed solution intake zone 203 is sent into concentration systems.
Four, reverse osmosis membrane and nanofiltration membrane are concentrated
Use reverse osmosis membrane concentrated parallel feeding district lower column liquid in anion-exchange resin column Continuous Moving Bed, it is that the nanofiltration membrane of 1～5nm is concentrated that the concentrated solution of reverse osmosis membrane re-uses aperture, obtain the lower column liquid of 22% concentration, it is again concentrated that the dialyzate of nanofiltration membrane is sent reverse osmosis membrane again back to.Concentrated solution is sent into the gel-type chromatographic separation resin column Continuous Moving Bed rotating counterclockwise.
Five, gel-type chromatographic separation resin column Continuous Moving Bed is separated
As shown in Figure 3, gel-type chromatographic separation resin column Continuous Moving Bed is provided with 20 resin columns, and is divided into successively in the direction of the clock D-ribose elution zone 301, prolongation disengaging zone 302, impurity disengaging zone 303 and assorted 304 4 subregions of sugared enrichment region with salt-free water elution.This wherein, 1st～No. 5 posts that are connected in series are D-ribose elution zone 301, enter feed liquid in one first batch can 1, the first batch can 1 enter and extend disengaging zone 302 from extending the ingress of disengaging zone 302 from the lower column liquid of D-ribose elution zone 301; 6th～No. 10 posts that are connected in series are for extending disengaging zone 302, the lower column liquid that extends disengaging zone 302 enters one second batch can 2, to the interior supplementary pending fresh concentrated solution of the second batch can 2, the mixing solutions in the second batch can 2 enters impurity disengaging zone 303 from the ingress of impurity disengaging zone 303; 11st～No. 15 posts that are connected in series are impurity disengaging zone 303, and the feed liquid that the lower column liquid of impurity disengaging zone 303 enters in one the 3rd batch can 3, the three batch cans 3 enters assorted sugared enrichment region 304 from the ingress of assorted sugared enrichment region 304; 16th～No. 20 posts that are connected in series are assorted sugared enrichment region 304, and the lower column liquid of assorted sugared enrichment region 304 is discharged as waste water.
The flow rate of liquid of D-ribose elution zone 301 is 62mL/min, and its import is arranged on the upper end opening for feed of No. 1 post, and its outlet is arranged on the lower end discharge port of No. 5 resin column; The flow rate of liquid that extends disengaging zone 302 is 45mL/min, and its import is arranged on the upper end opening for feed of No. 6 post, and its outlet is arranged on the lower end discharge port of No. 10 resin column; The flow rate of liquid of impurity disengaging zone 303 is 53mL/min, and its import is arranged on the upper end opening for feed of o.11 post, and its outlet is arranged on the lower end discharge port of No. 15 resin column; The flow rate of liquid of assorted sugared enrichment region 304 is 26mL/min, and its import is arranged on the upper end opening for feed of No. 16 post, and its outlet is arranged on the lower end discharge port of No. 20 resin column.
The feed liquid of collecting in the first batch can 1 is D-ribose product.
The turntable rotation cycle of controlling gel-type chromatographic separation resin column Continuous Moving Bed is 300min.
After turntable rotation two weeks, continuous moving bed system is balanced, detect the liquid material of the first batch can 1, the purity of D-ribose is 98%, the loss of D-ribose is minimum, by calculating charging D-ribose total amount and discharging D-ribose total amount, investigates material balance situation, result demonstration, D-ribose yield is 96.5%.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (1)
1. a method for purifying and separating for D-ribose, is characterized in that, comprises following step:
1) by D-ribose fermented liquid molecular weight cut-off, be that 10,000～15,000 flat sheet membrane is filtered, the filtered liquid of flat sheet membrane sent into the cation exchange resin column Continuous Moving Bed rotating counterclockwise;
2) cation exchange resin column of Continuous Moving Bed is divided in the direction of the clock successively to mixed solution intake zone, Xi Suan district and five, the acid regeneration district subregion of water liftout district, flat sheet membrane filtered liquid intake zone, Gai Shui liftout district liftout water and this intake zone lower column liquid, collect the outlet of parallel feeding district and remove cationic lower column liquid, lower column liquid is sent into the anion-exchange resin column Continuous Moving Bed rotating counterclockwise;
3) anion-exchange resin column of Continuous Moving Bed is divided into water liftout district, the mixed solution intake zone that removes cationic lower column liquid intake zone, Gai Shui liftout district liftout water and this intake zone lower column liquid, five of He Jian breeding blankets, soda district subregion in the direction of the clock successively, collects the lower column liquid that the outlet of parallel feeding district removes negatively charged ion;
4) lower column liquid in step 3 is concentrated into 18～25% concentration, then concentrated solution is sent into the gel-type chromatographic separation resin column Continuous Moving Bed rotating counterclockwise;
5) the gel-type chromatographic separation resin column of Continuous Moving Bed is divided into D-ribose elution zone, prolongation disengaging zone, impurity disengaging zone and the assorted sugared enrichment region with salt-free water elution in the direction of the clock successively, the lower column liquid of D-ribose elution zone enters the first batch can, feed liquid in the first batch can enters prolongation disengaging zone from extending the ingress of disengaging zone, then from extending the exit of disengaging zone, flows into the second batch can again; In the second batch can, supplement pending fresh concentrated solution, the mixing solutions in the second batch can enters impurity disengaging zone from the ingress of impurity disengaging zone, then from the exit of impurity disengaging zone, flows into the 3rd batch can again, and the feed liquid in the 3rd batch can is discharged as waste water; The feed liquid of collecting in the first batch can is D-ribose product;
Wherein,
The working pressure of flat sheet membrane is controlled at 1～6bar, and temperature is controlled at 20～60 ℃;
In step 2, water liftout district comprises 2～3 resin columns that are connected in series, flow rate of liquid is 25～35mL/min, intake zone comprises 2～3 resin columns that are connected in series, flow rate of liquid is 90～100mL/min, mixed solution intake zone comprises whole series connection, 4～5 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 110～140mL/min, Xi Suan district comprises whole series connection, 5～7 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 45～55mL/min, acid regeneration district comprises 4～6 resin columns that are connected in series, flow rate of liquid is 35～45mL/min, cation exchange resin column Continuous Moving Bed system amount of resin is 5～12L, the rotating disk cycle is 500～650min,
In step 3, water liftout district comprises 2～3 resin columns that are connected in series, flow rate of liquid is 25～35mL/min, intake zone comprises 2～3 resin columns that are connected in series, flow rate of liquid is 60～80mL/min, mixed solution intake zone comprises whole series connection, 4～5 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 90～110mL/min, soda district comprises whole series connection, 5～7 resin columns that all merging in parallel or in parallel is connected in series, flow rate of liquid is 50～70mL/min, alkali breeding blanket comprises 4～6 resin columns that are connected in series, flow rate of liquid is 35～45mL/min, anion-exchange resin column Continuous Moving Bed system amount of resin is 5～12L, the rotating disk cycle is 500～650min,
In step 4, use reverse osmosis membrane concentrated the parallel feeding district lower column liquid obtaining in step 3, it is that the nanofiltration membrane of 1～5nm is concentrated that the concentrated solution of reverse osmosis membrane re-uses aperture, obtains the lower column liquid of 18～25% concentration, and it is again concentrated that the dialyzate of nanofiltration membrane is sent reverse osmosis membrane again back to;
Several gel-type chromatographic separation resin columns of Continuous Moving Bed are divided into D-ribose elution zone, prolongation disengaging zone, impurity disengaging zone and assorted four subregions of sugared enrichment region in the direction of the clock successively, and the feed liquid in the 3rd batch can is entered to assorted sugared enrichment region from the ingress of assorted sugared enrichment region, then from the outlet of assorted sugared enrichment region, flow out, the feed liquid of outflow is discharged as waste water again;
In step 5, the feed liquid take-off rate of the second batch can is identical with the feed liquid of the second batch can inflow flow velocity;
In step 5, D-ribose elution zone comprises 5～6 resin columns that are connected in series, flow rate of liquid is 59～62mL/min, extend disengaging zone and comprise 5～6 resin columns that are connected in series, flow rate of liquid is 44～45mL/min, impurity disengaging zone comprises 5～6 resin columns that are connected in series, flow rate of liquid is 51～53mL/min, assorted sugared enrichment region comprises 5～6 resin columns that are connected in series, flow rate of liquid is 23～26mL/min, gel-type chromatographic separation resin column Continuous Moving Bed system amount of resin is 8～16L, and the rotating disk cycle is 200～300min.
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| CN102586492B (en) * | 2011-12-31 | 2015-04-22 | 三达膜科技（厦门）有限公司 | Method for removing impurities from saccharification solution in glucose production process |
| CN103073623B (en) * | 2012-12-28 | 2014-10-15 | 三达膜科技（厦门）有限公司 | Separation and purification method for colistin sulfate |
| CN104370978B (en) * | 2014-12-08 | 2016-07-06 | 山东润德生物科技有限公司 | A kind of method purifying D-ribose from D-ribose crystalline mother solution and device |
| CN104447889A (en) * | 2014-12-18 | 2015-03-25 | 郑州拓洋生物工程有限公司 | Preparation method of high-purity D-ribose |
| CN109225355B (en) * | 2018-11-13 | 2023-11-14 | 赛普特环保技术(厦门)有限公司 | Continuous ion exchange process for removing inorganic salt and system adopted by same |
| CN110368716B (en) * | 2019-07-31 | 2023-11-14 | 赛普特环保技术(厦门)有限公司 | Sugar and inorganic salt separation system and method |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2162721A (en) * | 1938-08-19 | 1939-06-20 | Claude S Hudson | Production of d-ribose from calcium d-altronate |
| US3380901A (en) * | 1963-08-07 | 1968-04-30 | Tanabe Seiyaku Co | Process for preparing d-ribose |
| US3970522A (en) * | 1973-11-23 | 1976-07-20 | Takeda Chemical Industries, Ltd. | Method for the production of D-ribose |
| CN1234404A (en) * | 1999-03-22 | 1999-11-10 | 华东理工大学 | Method for separating D-ribose from fermentation liquor |
| CN1359902A (en) * | 2000-12-22 | 2002-07-24 | 南开大学 | Process for preparing high-purity D-ribose from fermented glucose liquid |
| CN1508138A (en) * | 2002-12-18 | 2004-06-30 | 诚志生命科技有限公司 | Method for extracting D-ribose crystal from fermented broth |
| CN1616473A (en) * | 2004-09-21 | 2005-05-18 | 山东省食品发酵工业研究设计院 | Method for separating and extracting D-ribose from fermented liquid by film separating technology |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5416482B2 (en) * | 1974-03-15 | 1979-06-22 |
-
2010
- 2010-12-31 CN CN201010621589.9A patent/CN102241706B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2162721A (en) * | 1938-08-19 | 1939-06-20 | Claude S Hudson | Production of d-ribose from calcium d-altronate |
| US3380901A (en) * | 1963-08-07 | 1968-04-30 | Tanabe Seiyaku Co | Process for preparing d-ribose |
| US3970522A (en) * | 1973-11-23 | 1976-07-20 | Takeda Chemical Industries, Ltd. | Method for the production of D-ribose |
| CN1234404A (en) * | 1999-03-22 | 1999-11-10 | 华东理工大学 | Method for separating D-ribose from fermentation liquor |
| CN1359902A (en) * | 2000-12-22 | 2002-07-24 | 南开大学 | Process for preparing high-purity D-ribose from fermented glucose liquid |
| CN1508138A (en) * | 2002-12-18 | 2004-06-30 | 诚志生命科技有限公司 | Method for extracting D-ribose crystal from fermented broth |
| CN1616473A (en) * | 2004-09-21 | 2005-05-18 | 山东省食品发酵工业研究设计院 | Method for separating and extracting D-ribose from fermented liquid by film separating technology |
Non-Patent Citations (4)
| Title |
|---|
| JP特开昭50-123612A 1975.09.29 |
| 严滨，等.膜分离技术在D-核糖分离提取中的应用.《科技导报》.2009,第27卷(第11期),第52-55页. * |
| 于志萍,等.D-核糖提取精制的初步研究.《药物生物技术》.2003,第10卷(第4期),第242-244页. * |
| 张津枫，等.离子交换法提取D-核糖的研究.《离子交换与吸附》.2004,第20卷(第1期),第70-75页. * |
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